関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | 4-Chloromethyl-N-(2-methoxyphenyl)benzamide | HCID 19689968 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-(2-Methoxyphenyl)-4-dimethylaminomethylbenzamide | HCID 19690030 | 100% |
反応手順
In an atmosphere of argon, 4-chloromethyl-N-(2-methoxyphenyl)benzamide (276 mg, 1.0 mmol) was put into a 25 ml capacity eggplant type flask equipped with a cold finger and dissolved in dioxane (3 ml), followed by the addition of 50% dimethylamine aqueous solution (3 ml) at room temperature. After 2.5 hours of stirring at 80° C. and subsequent removal of dioxane by evaporation, the resulting residue was diluted with ethyl acetate (30 ml). The thus diluted solution was dried on anhydrous sodium carbonate, and the resulting residue was purified by subjecting it to a silica gel column chromatography (ether-ethyl acetate-ethyl acetate:methanol=10:1) to obtain 284 mg (100%) of the title compound in the form of colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728835 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-e6f09e6358c645c8a45e3f4af446ce3d |
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| 出典メモ | uspto-grants-1998_03 |
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